JPH07500007A - Clarified Konjac Glucomannan - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] Clarified Konjac Glucomannan The present invention substantially eliminates insoluble impurities, has low nitrogen content, and has low aqueous sol turbidity. Cleared or clarified konnyaku made from glucomannan derived from konnyaku. Concerning Nyaku and sol and gel made from it.

Konjac (Amorphophallus konjac) is a type of plant whose tuber power It is the source of a well-known food product in Okinawa and Japan: konnyaku flour. this The fine powder contains various insoluble substances listed below as well as large amounts of desirable water-soluble substances. and when reconstituted with water forms a highly viscous sol of glucomannan and soluble starch do. The main soluble components are glucomannan, D-glucose and D-mannose This component is useful as an ingredient in various foodstuffs. as well as industrial components such as films, oil drilling fluids and coatings. It is useful as

Crude (natural, unclarified) konjac powder contains many impurities, mainly insoluble Nitrogen-containing substances are present, including flour, cellulose and proteins.

Many of these impurities are found in the sac that encloses the konnyaku powder inside the tuber. It arises from As a result, the sol and gel of crude konjac powder (water have a markedly cloudy, milky or cloudy appearance (attributable to expanded particulate impurities). One.

Sugiyama et al., U.S. Pat. No. 3,928,322 (and its sequel, U.S. Pat. No. 3,973,008 first filters insoluble impurities from an aqueous konjac powder sol. by filtration or other conventional methods, then dialyzing the sol and obtaining The liquid is freeze-dried to produce a cloudy cotton that is difficult to grind and hardly soluble in water. mainly from crude konjac powder by obtaining a low-density fibrous product with Konjac mannanbo saccharide consisting of konjac powder, i.e. glucoman It describes a method for producing naan.

Japanese Unexamined Patent Publication No. 1-49657 (published on March 1, 1989) has a nitrogen content of less than 0.02%. A konjac mannan product containing elementary components is described. However, this The method to achieve reduced nitrogen content is not described, but it is It is clear that this is due to dilution.

U.S. Pat. No. 2,144,522 discloses that a gummy sol is prepared in the presence of aluminum sulfate. Locust bean gum (locust bean) is prepared by contacting it with activated carbon. Describes a method for decolorizing and clarifying galactomannan gum sol such as gum) are doing. Aluminum sulfate is originally a double salt with sodium sulfate that exists in activated carbon. Added in sufficient amount to form Al-Na.

U.S. Pat. No. 3,346,556 discloses that galactomanganese produced by heat or pH change A method for preventing the decomposition of naan, such as locust beans, is described. This method Polar organic oxygen-containing hydrophilic stabilizers, such as alcohols, glycols, and or the like. Along with this method, diatomaceous earth One practice is to clarify locust bean gum by the regular use of filter aids. Example (Example 5).

JP-A-59-227,267 (published on December 20, 1984) and 58- No. 165,758 (published on September 3, 1983) is an aqueous solution of crude konjac powder. The sol is treated with some kind of salt at a pH of 10 or lower to remove mainly insoluble food. describes a method for obtaining konnyaku in insoluble form for use as a commercial product. Ru.

Japanese Patent Application Laid-Open No. 63-68054 (published on March 26, 1988) discloses a reversible soluble copolymer. Nnyaku gel product is described, but removal of insoluble substances that remain in the product is not listed.

Is it a combination of glucomannan obtained from crude konjac and other hydrocolloids? Gums formed from ids are already known in the art. For example, U.S. Pat. Known as No. 27,704.

The present invention substantially eliminates insoluble impurities, and the nitrogen content is less than about 0.60 wt%. Formazin Turbidity3 standard ) using the concentration 1. Aqueous sol turbidity potential measured in Ow/v% is 20 turbidity Clarified konnyaku consisting of glucomannan derived from konjak that is smaller than the unit Provides a method for producing the same.

The "clarified" konnyaku used here is one that has been clarified without substantially eliminating insoluble impurities. Not clarified in the form of an aqueous sol or gel with a lower nitrogen content than konjac. No konjac glucomannan exhibits lower turbidity than konjac. used here "Crude" konnyaku contains naturally occurring glucomannan that is still contained in the sacs. Refers to unclarified or natural konnyaku powder, which may contain various other impurities. .

The clarified glucomannan product of the present invention is produced by dispersing konjac flour in water and dispersing the resulting By treating the dispersion with a salt such as aluminum sulfate to extract the impurities present, can be obtained. These impurities are mainly naturally occurring from konjac tubers; For example, nitrogenous substances such as proteins, or insoluble fibers, feces, etc. of extraction After that, impurities are separated from the sol, and a water-miscible coagulant such as alcohol is added to the remaining sol. The glucomannan is coagulated, and the resulting coagulated product is dried and crushed to form a powder. this Improved production by adding other ingredients such as food ingredients when dissolving the dry powder in water. It can be made into a product. This method is significant in that it can be done much faster than conventional methods. There are great advantages.

The method of the present invention provides unclarified (crude) konjac powder with improved odor, Provides additional benefits such as color, solubility and grindability. Crude konjac paste If you smell it, it has a tan skin or dark brown color (in powder form). Also, raw konnyaku Yakuza particles are non-uniform in size and cannot be ground at normal grinding temperatures. crude konnyaku The grinding process generates high temperatures that destroy viscosity and darken the color, similar to dry thermal decomposition. bring about On the contrary, the clarified konnyaku of the present invention is a white powder and forms a transparent sol. It is odorless and easy to grind to a uniform size. Konya has also become transparent. konnyaku has a more uniform gum content and a wider range of viscosity and gel strength than crude konjac. can prevent uncontrollable changes.

Further superior properties of the clarified konjac powder of the present invention are that it is different from crude konjac powder. It hydrates easily by just putting it in water at room temperature without much effort, thereby Promote the use of konnyaku in various food formulations and in the production of sols and gels.

Figure 1 shows the nitrogen value and turbidity value of the composition of the present invention compared to the nitrogen value and turbidity value of the conventional product containing crude konjac. Figure 2 is a graph comparing the values and turbidity values.

Unless otherwise specified in the operational examples or elsewhere, the amounts of ingredients, parameters, or The numbers indicating reaction conditions are accompanied by "about" in each case.

Crude konjac starting material The crude konjac powder starting material is an industrial product available from a number of sources.

One raw material and method for producing konjac powder is marine colloid plutin-1 (Marine Co11oids Bulletin K-1), rNUTRI COL■ Konjac FlourJ (1989) (FMC Corporation Marine Co11oids Division, Marine Products and Reports Philadelphia, Pennsylvania! 9103, U, S, A) . Basically, this method uses Amorphophallus tubers (Amorphophallus tubers). US tuber) is sliced, dried and wet or dry milled, then The konnyaku obtained in Including crushing. As described in the above-mentioned literature, the obtained powder has fine particles. , consisting of oval, whitish "powder sac"-containing particles. That is, gluco The mannan is encapsulated in a protein/fiber coating. This fine powder is When stirred and hydrated over time, the encapsulated glucomannan is released and the 1% Even at concentrations of form a le. 8,000 cps for 1 wt% sol to 130,00 cps for 3 wt% sol Brookfield ORVT has a viscosity in the range 0. a viscometer and a suitable spindle at 20 rpm and 25°C (the viscometer is a Brookfield Field Engineering Laboratories, Inc., Sto. ughton, Mass.

, U, S, A), heating (85°C) and cooling service. Exemplary obtained after the cycle. Brookfield Centipoise (Cps) Conversion of readings to viscosity functions is provided in Rheologica Acta, 2. here When used in centipoise (cps), centipoise (cps) is millipascals second (mP- s).

Crude konjac turbidity varies significantly depending on the concentration of the sol, but at 8,000 cp In the aforementioned viscosity range of s to 130.00'0 cps and concentration of 1% to 3%, 1 A turbidity of 00 to 300 turbidity units is determined according to the Formazin turbidity standard ( FTS) (EPA Environmental M.

Nitoring and 5upport Lab; March, 1979 "Method of Chemical Analysis of Water End" According to method 180.1) of ``Tez'', it is usually obtained at a concentration of 0.5 wt%. . At these turbidities, the sol generally appears cloudy and very cloudy.

The high nitrogen content of early crude konnyaku powder was essentially due to impurities, mainly due to the natural origin of the tubers. It is a function of the amount of sac fibers that envelop the sack and glucomannan. dry coarse flour The nitrogen content at the end can be high depending on the type of tuber used. However, a range of 0.3 to 1.3 wt% nitrogen is typical.

As shown in the figure, the 1.0% aqueous sol of the clarified konjac of the present invention is formed by Formazine. Macbeth Co1orey computer using the standard Model 1500 with New York New Bar 7 (7)K.

11morgen Corp.) is less than 20 turbidity units. stomach.

The clarified konjac of the present invention preferably has a content of 0.60 wt% or less, regardless of its form. preferably 0.25 wt% or less, more preferably 0.175 wt% or less, most preferably has a nitrogen content of less than 0.15%.

The clarified konjac sol of the present invention having these ranges is transparent in appearance, transparent and granular. Foods and other products where a childless gel is required or a highly viscous material is desired. It can be used in many fields.

The clarified konjac of the present invention further comprises a clarified konjac/aqueous sol of 1°Ow/v. % viscosity at 25 °C using a Brookfield viscometer model LVTDV-II, It is characterized in that it is approximately 1,000 to 25,000 cpS when measured at 20 rpm. It is a sign.

Turbidity of powder and product samples is commonly measured using visible light; Ultraviolet (UV) light is used to characterize materials and measure the effectiveness of clarification methods. child To do this, make a 0.5% aqueous sol of the product and place it in a cuvette at 200 and 32 This can be done by measuring UV light absorbance between 0 nanometers (nm). . Impurities including DNA and proteins absorb UV light at 260-280 nm, and this Area peaks indicate their presence and relative abundance. Crude samples are spread over this area. The absorbance is higher than that of the clarified sample, which has a 260-280 peak and no 260-280 peak. baseline or higher.

Crude 0.5140 0.8781 0.9634 2.6115 Clarification 0,0647 0.0967 0.1222 0.3118 Method description The method for producing clarified konjac of the present invention consists of the following steps.

(a) of crude konjac containing insoluble impurities, starch and glucomannan; Create an aqueous sol, (b) Add this crude konjac sol to dicalcium phosphate, calcium phosphate, phosphorus of an extraction salt selected from one or more of magnesium acid (preferably aluminum sulfate). (C) contacting with an amount effective to extract insoluble impurities by precipitation; letting it settle, separating the insoluble impurity precipitate (by filtration, etc.) and discarding it; (d) Remove the remaining aqueous sol using C1 such as methanol, ethanol or 2-propanol. -4 Lower alcohols or water-miscible polar organic solvents such as acetone and methyl ethyl ketone from a sol of one or more water-miscible coagulants selected from a solvent or a mixture thereof. Process the glucomannan in a sufficient amount to solidify it to form a glucomannan solidified product. and then (e) separating and drying the glucomannan coagulum to obtain clarified glucomannan. Collect mannan.

"Extraction" here refers to removing insoluble impurities from konnyaku by coagulation, adsorption, or precipitation. It means excluding. Dicalcium phosphate, calcium phosphate and magnesium phosphate Aluminum sulfate or extraction salts were found to be the most effective, although aluminum is also effective. other water Miscible coagulants are also effective, but isopropyl alcohol is the most effective coagulant. That's what I found out. The coagulant can be dried and ground into granules using known methods. Ru.

The individual steps and conditions of the invention may vary somewhat. Generally speaking, one or more draws The salt is mixed with the crude konjac powder starting material and optionally a filter aid; Disperse the dry mixture in sufficient amount of water under stirring to obtain the crude glucomannan-containing glucomannan concentration. Make Nnyakusol. The concentration depends on the viscosity or 01 = 10 wt%, more preferably is 0.5 to 3 wt%.

Alternatively, one or more extraction salts may be added to the water before or after the aqueous dispersion of the crude konjac. . This dispersion can be carried out in water at room temperature, but preferably at 70-100°C, preferably at 85-100°C. Heating the water to 90°C for 15-60 minutes is preferred to speed up the process. warm The temperature, mixing ratio, and concentration should be determined by a person skilled in the art to optimize these operating conditions. Return as appropriate.

The filtration step removes insoluble impurities and may be performed by adding a filter aid.

Filters such as glass wool, paper, cloth, and fibrous mats can be used for this purpose. Of course, any filter can be used as long as it can sufficiently remove insoluble particulate matter. stomach. Examples of filter aids include perlite and diatoms. The amount of filter aid is critical It is preferable that the amount is 1 to 5 times that of crude konjac powder. Then the filter Add the clarified konjac glucomannan to the heated water until it is no longer recovered. Washing is preferred.

Examples of water-miscible coagulants preferably used in the present invention include methanol, ethanol, CI-4 lower alcohols such as alcohol or 2-propanol, acetone, methyl ethyl water-miscible polar organic solvents such as ketones or mixtures thereof; sopropyl alcohol) is more preferred. The amount of coagulant added is not critical but at least enough to recover glucomannan as a coagulum from the remaining sol. The amount should be effective for coagulation. Preferably, the coagulant:glucomannan weight ratio is The volume ratio is 1 to 4:l or 2 to 3:1.

It is preferable to dry the coagulated material until it can be ground into fine powder. This is an analogy For example, it can be carried out in a hot air oven at ambient temperature. Then the dry product Grind into granules of desired size. Preferably, for example, 100 metunyu (1 The powder is ground to obtain a fine powder that passes through a 49 micron sieve.

The easy solubility of the clarified konnyaku of the present invention is that of the starting material before clarification subjected to the method of the present invention. This is one of several distinguishing characteristics. The desired concentration % of this composition in the sol is mainly depends on its intended use and viscosity. As mentioned above, based on the sol weight, 0.1 ~10 wt%, preferably 0.5 to 3.0 wt% is used, but this amount is critical Not the point. Also, some of the processing steps mentioned above typically maintain very high viscosities. However, it is particularly preferred for food applications.

This sol was also measured using a Brookfield viscometer model LVTDV-II. Viscosity measured at 25°C, concentration 1.0 w/v%, spindle rotation speed 2 Orpm Not only does it have a high viscosity, usually 1,000 to 25,000 cps, This viscosity can be quickly achieved due to the fast hydration properties of this clarified dry powder. It also has the characteristic of being In other words, regular unclarified konjac powder is mixed with water. To make a 1wt% sol by dispersing the The hydration time for the product of the invention is approximately 2 hours or less under substantially the same conditions. The total time is approximately 30 minutes.

The substantially transparent gel thus obtained is purified by a known method for gelling konnyaku. Converted to clarified konnyaku gel. For example, gelation of known gelling agents for konjac. An example of this method is to mix an effective amount of the compound at a known temperature.

If desired, the extraction salt may be formed in situ during the extraction process by known methods. I can do it. The amount of these salts is not critical but sufficient to coagulate the glucomannan. The amount is preferably 1 to 25 wt% based on the weight of the crude konjac. , more preferably 5 to 15 wt%.

The amount of clarified konjac used as an additive to food or industrial compositions is essentially The advantages of the present invention are in its purity, appearance and hydration properties. Ru. For example, 0.1 wt% is used in cake mixes, film, oil Amounts of 1-2% or more are used in industrial applications such as rill fluids and paints. Ru.

Example 1 (dicalcium phosphate) 600 ml of distilled water was heated to approximately 75-78°C in a hot water bath. Dical phosphate Add 0.6g (lOw/w% of crude konjac) of Si to this hot water as an extractant. I got it. Next, add 6g of crude konnyaku (FMC lot number 89-9609) and do the same. Stirred for 60 minutes while maintaining temperature. After this “cook” treatment, 15 g of filtration Auxiliary agent (rcelatonJ diatomaceous earth) 1 Cincinnati, Io Eagle P Itcher Industries Inc.) and fill with the same dimensions. Filtration was carried out in an If pressurized filter cylinder equipped with a turquoise only. this The filter cylinder was preheated with boiling water and the preheating water was removed. Sample this Put it in a filter cylinder and apply a pressure of 25 ps (1.75 kg/cm2) to 10 It took a minute. Then, increase the pressure to 40 ps i (2.8 kg/am") This pressure was maintained for 40 minutes. During this time only 50 ml of filtrate was collected and sampled. Remove the filter from the filter cylinder, combine it with this small amount of filtrate, and add the filter aid 8. 5g was mixed. The filter cylinder was cleaned, reassembled, and preheated. with the following times Repeated pressure filtration for 110 minutes 10 psi (0.7 kg/cm2); 30 minutes 2 5psi (1,75kg/am2); 60 minutes 40psi (2,8kg/cm2) ”) and 10 minutes at 60 psi (4,2 kg/cm”) o Total filtration time is 120 minutes During this time, 250 ml of filtrate was collected. The filtrate was diluted with 2 volumes of 99% 2-propatool. The mixture was allowed to solidify and left for 60 minutes. The coagulum was collected by vacuum filtration and lyophilized to double the volume. 60% of 2-propertool for 30 minutes.

The coagulum was collected again and dried in a hot air oven at 50”C overnight (14 hours). Ta. Weigh this sample (1.65 g or 27.4% yield) and pass through a 4° mesh sieve. It was crushed until it passed through. Brookfield Digital Viscometer Model LVTDV- The 1% viscosity of the product measured at 25 °C using an It,Nα1 spindle is 4,4 It was 10cps.

Example 2 (aluminum sulfate) Following the method of Example 1, instead of dicalcium phosphate 0.6 g aluminum sulfate was added to konnyaku. After 35 minutes, 500 ml of filtrate was collected and treated similarly. . The dried sample, 3.15g or 52.6%, was ground to 1% sol and gel. It was used to make. The viscosity measured using the same measurement parameters is 2.17 It was 0cps.

Example 3 (Aluminum sulfate made in situ) was added to 600 ml of distilled water under stirring. ．． Add 747 g monobasic sodium sulfate and 0.847 g aluminum chloride. Ta. l without filter aid.

After minutes, 500 ml of filtrate was collected at 5 ps i (0.35 kg/cm").

The product was treated in the same way, dried, and ground to give 4.20 g (70% yield) of the desired product. Obtained. The product had a viscosity of 1% or 1%, measured using the same measurement parameters as in Example 1. ,720cps.

Example 4 (Aluminum sulfate made on the spot) The above extraction was carried out by adding some conditions. repeated. In this example, 0.526g (7) aluminum chloride (anhydrous AlCl, 0.291 g) and 0.310 g of monobasic sodium sulfate were used. Further filtration 25g of filter aid was added beforehand. After 98 minutes, 450 ml of clear filtrate was collected and treated as before. It was processed like this. After drying, 3.65g (yield 60.9%) of the product was ground to form a 1% sol. was used to generate This sol is highly transparent and can be measured using the same measurement parameters as in Example 1. The measured viscosity was 1,150 cps.

Example 5 (dicalcium phosphate made in situ) with 0.694g of calcium chloride 0.567 g of monobasic sodium phosphate was used for extraction. without using filter aids, 340 ml of filtrate was collected and treated in the same manner to obtain 2.90 g (yield 48.3%) of product. Obtained. The 1% viscosity of this sample measured using the same measurement parameters as in Example 1 is 17,000 cp 225 gallon (approximately 852 f) stainless steel tank, 140 gallons (53017) cold water, 214 g aluminum sulfate (4.71%) ) and 162 ml of 3M NaOH were added and heated to 70°C with direct steam. 10 Pounds (4536g) 0) yak powder and 31 pounds (14062g) +1 7) Mixed with FW40 filter aid. Total volume is 160 gallons (60612) This corresponded to 0.75 w/v% of Nyaku. Heat this sample to 85°C and hold for 15 minutes. I held it. This sample was then placed in a preheated 18 inch (46 cm) stainless steel The first 5 minutes were recycled and filtered using a filter press. filter Filtration time, including time to flush the press with hot water, was 60 minutes. 300 Coagulate the filtrate in a gallon (1,136 f) of 85% isopropyl alcohol IPA I let it happen. The coagulum is screened and compressed through a bag and then in a small press. It was squeezed with The coagulum was then washed with air using 75 gallons (284 f) of 85% PA. Washing/curing was performed while stirring.

The coagulum was screened and then manually squeezed to remove excess liquid and kept at 55°C overnight. Dry. This sample, 6.4 bond (2,9 kg) or yield 64%, was 0. The powder was ground through a 0.039 inch (2.4 mm) screen.

Nitrogen content 0.15%, 1% turbidity II NTU (Nephelometric T It was urbidity units).

Examples 8 to +9 (Nitrogen content and turbidity of clarified konnyaku) The nitrogen content and turbidity level of the product was measured (Examples 8-II). These results can be roughly Konjac Powder, (Examples 13 and 15-19) and U.S. Patent No. 3,928,32 The product obtained by the method described in No. 2 (Example 12) and “Biophysics 431.155-15 Described in "Electrophoresis for Konjac Mannan Gel", page 8 (1987) The product of Ogasawara et al. (Example 14) (here, part of U.S. Pat. Nitrogen content and turbidity levels were compared with the nitrogen content and turbidity levels of different methods (as indicated).

The full results of these tests are shown in Table 1 and Figure. Total nitrogen values are based on dry weight of product. It is something that can be developed.

In Table ■, as stated in Note (b), some of the turbidity values are - Spectrophotometer model (Pittsburgh, Pennsylvania Fisher 5cie) ntific) using the Formagin standard. converted to a value. This conversion was performed as follows. Range of 5-40ONTUs Created 11 Formagine standards with turbidity values, including both Macbeth and Fisher units. (Transmittance %) was measured for each person.

We also added five konjac samples (crude 3 clarified 2) to 1%, 0.5%, and 0.25%. and 0.125% and measured in hundreds. From these measurements The obtained data (transmittance %) is then plotted against the turbidity value and the measured correlation coefficient. I did it.

The method of U.S. Pat. No. 3,928,322 - Sugiyama (Example 12) was carried out as follows. .

1.2.5g of konnyaku powder (89-9607) in 500ml (0°5W/ V%) in tap water and heated at 55-60°C for 2 hours.

2. 115 meshes (125 microns) of this sol, then 270 meshes (5 microns) The mixture was passed through a metal screen (3 microns) to remove larger insoluble matter.

3. This sol is a medium porosity glass filter (Pyrex 150ml, AS TM 1O-15) or 0.2 micron filter; Instead, heat it to 90℃ and make a 14 inch - 1 inch diameter (35°6cm - 3,54cm). diameter) twice through a tightly backed glass wool bed. 300ml of filtrate is High transparency (no particles observed).

4. Pour the filtrate into a piece of dialysis tube (Spectra/Por, 47.7mm x 75 mm, molecular weight cut of 12->14,000 daltons). The sample Dialysis was performed for 48 hours against 41 tap water (the water was changed after 24 hours).

5. The samples were poured into two crystallization dishes and frozen.

6. Freeze-dry each component in a bath temperature of 100°F (37.8°C) at 0.6 Torr. It was dry. The dried sample was very white and very soft. Yield: 1゜137g The rate was 45.5%. A small amount of 20% isopropylene cannot be crushed due to excessive static electricity. It was moistened with lopyl alcohol and then dried at 55° C. for 3 hours. Then sample 4 It was ground to pass through a 0 mesh screen.

The sample had a nitrogen content of 0.07% and a 0.5 turbidity of 66 turbidity units. . This method required 68 hours.

The Ogasawara method (Example 14) was carried out as follows.

1. Suspend 10g of crude konnyaku in 100ml of 50% ethanol for 1 week. Stirred.

2. Centrifuge this material and transfer the pellet to 100 m 180% ethanol for 3 days. Stir for a while.

3. Centrifuge this again at 4000 rpm for 10 minutes) and transfer the pellet to 100ml Transferred to 100% (absolute) ethanol and kept for 1 hour.

4. Collect this sample on a Ma54 Whatman filter by vacuum filtration.6 It was dried in a 0°C oven for 6 hours.

5. To collect 8.992g of this substance and create a 5% concentration sol in 178ml Using. This has a viscosity that is difficult to handle, and it can be diluted 10 times to 1780ml (0, 5 w/v%) and left at room temperature overnight.

6. This material was centrifuged at 9500 rpm for 75 minutes.

7. The supernatant (1700 ml) was dialyzed against 10 volumes of distilled water at room temperature for 10 days.

8. Remove this sample from the dialysis tube and centrifuge at 7500 rpm for 10 minutes. separated.

9. Solidify half of the supernatant and put the other half into a dialysis tube and insert it into a polyethylene tube. Cover with recall (PE020) and reduce the volume from 850m1 to 450m1 Ta.

10. Freeze this material at -75°C for 45 minutes and ITorr 100°F ( Freeze-dried at 37.8°C for 3 days.

2.19 g of this freeze-dried product was recovered. This was extremely white and had a soft appearance. .

12. All samples were vacuum dried to remove moisture before testing. For turbidity measurement as a sol The lyophilized product foamed excessively when prepared.

13. This method required a total of 384 hours.

Table■ invention 8 A1. Pilot plant 0.07 79 AI, pilot plant 0.07 1810 Al, pilot plant 0.15 11’″111 AI, pilot plant 0.13 14 Conventional example 12 Sugiyama Patent 0.07 128”’13 Crude/Hydro, Washed 0.11 17714 Ogasawara method 0.31 80Lb’15 Crude 0.32 92” ’ 16 Crude 0.30 101 17 Crude 0.29 120 18 Crude 0.4] 155”’ 19 Crude 0.59 142 (a) Samples were centrifuged at 400 rpm for 5 minutes before analysis.

(b) This value was originally obtained with a Fischer spectrophotometer and measured with the same instrument. It was determined by the regression line obtained by plotting the values obtained from the relative consideration of pull. Converted to Macbeth corresponding value.

(C) Product dry weight basis.

(d) Using the Formagin standard, Macbeth's Calligraphy Computer Measured at 500).

(e) Measured at Iw/v%, all others measured at 0.5w/v%.

From the above results, the nitrogen content and turbidity values of the products of the present invention (Examples 8 to 11) are both low, and the crude copolymer The corresponding values for Nnyaku, as well as for one or both of the Sugiyama and Kozutsu originals, are relative. was extremely high.

“　’)”’7’-’J? N 1xtQfa +3py-() Procedural amendment February 17, 1994

Claims (9)

[Claims] 1. Contains glucomannan derived from konjac and is substantially free of insoluble impurities. with a nitrogen content of about 0.60 wt% or less and using the Formazine turbidity standard. The aqueous sol turbidity potential measured at a concentration of 1.00 w/v% is 20 turbidity units. Clarified konnyaku characterized by its smaller size. 2. The clarified konnyaku according to clause 1, having a nitrogen content of 0.25% or less. 3. The clarified konnyaku according to paragraph 1, having a nitrogen content of 0.175% or less. 4. The clarified konnyaku of item 1, item 2 or item 3 comprising an aqueous sol. 5. The clarified konnyaku according to item 1, item 2 or item 3, comprising an aqueous gel. 6.1.0 w/v% clarified konjac/water sol has Brookfield viscosity The viscosity measured at 25°C and 20 rpm using a meter model LVTDV-II is approximately 1. The clarified konnyaku of paragraph 1 which is from 000 to 25,000. 7. (a) Aqueous solution of crude konjac containing insoluble impurities and glucomannan create a le, (b) The crude konjac sol is mixed with dicalcium phosphate, calcium phosphate, phosphoric acid. For precipitation of extraction salts selected from one or more of magnesium and aluminum sulfate (c) precipitating the insoluble impurities; (d) the remaining aqueous sol is freed from substantially all of the glucomannan therein; Glucomannan is coagulated by treating it with a sufficient amount of isopropyl alcohol to coagulate the glucomannan. make things, and (e) Glucomannan clarified by separating and drying the glucomannan coagulum 1. The method for producing clarified glucomannan according to item 1, which comprises recovering naan. 8. 7. The method of item 7, wherein the extraction salt is aluminum sulfate or calcium sulfate. 9. The method of paragraph 7, wherein the extraction salt is aluminum sulfate.